CN109796770B - Preparation method of flexible ablation-resistant composite material of three-source expansion micro-foaming flame-retardant system - Google Patents
Preparation method of flexible ablation-resistant composite material of three-source expansion micro-foaming flame-retardant system Download PDFInfo
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Abstract
The invention provides a preparation method of a flexible ablation-resistant composite material of a three-source expansion micro-foaming flame-retardant system, wherein the flexible ablation-resistant composite material is prepared from the following raw materials in parts by weight: 100 parts of silicone rubber, 5-20 parts of white carbon black, 3-20 parts of fiber, 5-60 parts of acid source substance, 5-60 parts of gas source substance, 5-60 parts of carbon source substance, 2-10 parts of curing agent and 0.2-2 parts of catalyst. The flexible ablation-resistant composite material prepared by the invention has excellent heat resistance and ablation resistance and good heat insulation performance, can be used for preparing ablation heat-resistant materials and parts with the requirements on heat resistance and ablation resistance, and is applied to the protection and sealing of structures and parts which need to withstand high-temperature gas, pneumatic heat flow scouring and other severe environments in aerospace aircrafts and related equipment.
Description
Technical Field
The invention relates to the field of composite materials, in particular to a preparation method of a flexible ablation-resistant composite material of a three-source expansion micro-foaming flame-retardant system.
Background
The ablation-resistant material generates a series of physical and chemical reactions under the condition of gas scouring, such as heat desorption, mass ejection effect of pyrolysis gas, re-radiation of a surface carbon layer and the like, can take away a large amount of heat, reduce the temperature of the protected material and prevent the material from further ablation and damage, and the ablation heat-resistant material has irreplaceable key effects in a space vehicle. With the development of aerospace craft towards faster speed, stronger maneuverability and more complex structure, the traditional rigid heat-proof ablation-resistant material can not completely meet the application requirements, the flexible ablation-resistant material plays an increasingly important role, and plays an increasingly important role in the thermal protection and sealing of some dynamic and complex connecting structures and the matching of large deformation and thermal stress, but the ablation resistance of the conventional flexible material is poor. With the further development of aerospace technology, the development of flexible thermal protection materials with excellent heat resistance, ablation resistance, scouring resistance and other properties has very important significance.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a flexible ablation-resistant composite material of a three-source expansion micro-foaming flame-retardant system, wherein the flexible ablation-resistant composite material is prepared from the following raw materials in parts by weight: 100 parts of silicone rubber, 5-20 parts of white carbon black, 3-20 parts of fiber, 5-60 parts of acid source substance, 5-60 parts of gas source substance, 5-60 parts of carbon source substance, 2-10 parts of curing agent and 0.2-2 parts of catalyst.
Further, the flexible ablation-resistant composite material is prepared from the following raw materials in parts by weight: 100 parts of silicone rubber, 15 parts of white carbon black, 12 parts of fiber, 10-50 parts of an acid source substance, 10-50 parts of a gas source substance, 10-50 parts of a carbon source substance, 3 parts of a curing agent and 0.2 part of a catalyst.
Further, the flexible ablation-resistant composite material is prepared from the following raw materials in parts by weight: 100 parts of silicon rubber, 15 parts of white carbon black, 12 parts of fiber, 40 parts of acid source substance, 40 parts of gas source substance, 10 parts of carbon source substance, 3 parts of curing agent and 0.2 part of catalyst.
Further, the silicon rubber is room temperature vulcanized liquid silicon rubber modified by epoxy resin.
Further, the preparation method of the epoxy resin modified room temperature vulcanized liquid silicone rubber comprises the following steps:
(1) heating epoxy resin and an organic silicon intermediate in an equimolar ratio to 105-155 ℃ under the condition of nitrogen, stirring, dripping 0.1-0.9 wt.% tetraisopropyl titanate after uniformly stirring, and stirring for 5-12 hours to obtain a reaction product;
(2) and adding 10-40 parts of the reaction product into 100 parts of a liquid silicone rubber matrix, uniformly mixing at 100 ℃, and cooling to obtain the silicone rubber.
Further, in the step (1), the epoxy resin is bisphenol A type epoxy resin; the organosilicon intermediate is polymethylphenylsiloxane; and/or in the step (1), the amount of the tetraisopropyl titanate is 0.1-0.9% of the weight of the organosilicon intermediate; and/or in the step (1), the rotating speed of stirring is 400-1000 r/min.
Further, the fiber is aramid fiber, PBO fiber, quartz fiber or carbon fiber; the acid source substance is ammonium sulfate, ammonium chloride, ammonium phosphate salt or borate; the gas source substance is ammonium borate, dicyandiamide, melamine or glycine; the carbon source substance is pentaerythritol, polyamide, thermoplastic polyurethane, phenolic resin or triazine derivative; the curing agent is a silane coupling agent; the catalyst is an organic tin compound.
Further, the fibers are PBO fibers; the acid source substance is ammonium sulfate; the gas source substance is ammonium borate; the carbon source substance is pentaerythritol.
Further, the preparation method comprises the following steps:
(a) weighing the raw materials according to the weight ratio of any one of claims 1 to 3;
(b) gradually adding a small amount of white carbon black into the silicone rubber, and uniformly mixing to obtain a silicone rubber white carbon black mixture; then sequentially and gradually adding the fiber, the acid source substance, the gas source substance, the carbon source substance and the curing agent into the silicon rubber and white carbon black mixture, and uniformly mixing; finally, adding a catalyst, mixing for 1-5 min, and uniformly mixing to obtain uniformly mixed raw materials;
(c) and putting the uniformly mixed raw materials into a mold, vulcanizing, demolding, sampling, and standing at room temperature for a week to completely cure the raw materials to obtain the product.
Further, in the step (b), the stepwise small-amount addition is a stepwise small-amount addition in a batch; and/or, in the step (b), the step-by-step adding in sequence means that after each same component is added, the other component is added after the same components are uniformly mixed; and/or in the step (c), vulcanizing in a vulcanizing press for 8-36 hours at room temperature and under the vulcanizing pressure of 5-15 MPa.
The acid source substance is also called dehydrating agent or charring accelerant, which is inorganic acid or compound that can generate acid in situ during burning, such as phosphoric acid, boric acid, sulfuric acid and phosphate.
The gas source substance is also called a foaming source and is a nitrogen-containing compound, such as urea, melamine, polyamide and the like, and the gas generated by the gas source substance expands and foams a molten system to form the porous carbon layer.
The carbon source substance is also called as a carbon forming agent, which is the basis for forming a foam carbonized layer and mainly comprises polyhydroxy compounds with high carbon content, such as pentaerythritol, phenolic resin and the like.
The flexible ablation-resistant composite material prepared by the invention has excellent heat resistance and ablation resistance and good heat insulation performance, can be used for preparing ablation heat-resistant materials and parts with the requirements on heat resistance and ablation resistance, and is applied to the protection and sealing of structures and parts which need to withstand high-temperature gas, pneumatic heat flow scouring and other severe environments in aerospace aircrafts and related equipment.
Obviously, many modifications, substitutions, and variations are possible in light of the above teachings of the invention, without departing from the basic technical spirit of the invention, as defined by the following claims.
The present invention will be described in further detail with reference to the following examples. This should not be understood as limiting the scope of the above-described subject matter of the present invention to the following examples. All the technologies realized based on the above contents of the present invention belong to the scope of the present invention.
Drawings
Figure 1 is a graph of line ablation rate results for different flexible ablation resistant composites.
FIG. 2 is an optical surface topography of the flexible ablation-resistant composite material of the present invention after ablation.
FIG. 3 is an SEM image of the ablated surface of the flexible ablation-resistant composite material of the invention.
FIG. 4 is an SEM image of a cross-section of a flexible ablation-resistant composite material of the present invention after ablation.
FIG. 5 is an X-ray diffraction pattern of the flexible ablation-resistant composite material of the present invention after ablation.
Fig. 6 is a graph of thermal conductivity results for different flexible ablation-resistant composites.
Fig. 7 shows the maximum back plate temperature results for different flexible ablation resistant composites.
Detailed Description
Examples 1-5 preparation of Flexible ablation-resistant composites of the invention
1. Raw material ratio
TABLE 1 raw material ratios of examples 1 to 5 of the present invention
| Raw materials (parts) | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| Silicone rubber | 100 | 100 | 100 | 100 | 100 |
| White carbon black | 15 | 15 | 15 | 15 | 15 |
| PBO fiber | 12 | 12 | 12 | 12 | 12 |
| |
30 | 20 | 10 | 50 | 40 |
| |
30 | 50 | 20 | 10 | 40 |
| Pentaerythritol | 50 | 40 | 20 | 30 | 10 |
| Curing agent | 3 | 3 | 3 | 3 | 3 |
| Catalyst and process for preparing same | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
In table 1, the silicone rubber is an epoxy resin modified room temperature vulcanizing liquid silicone rubber, and the preparation method thereof is as follows: adding bisphenol A type epoxy resin and polymethylphenylsiloxane in an equimolar quantitative ratio into a three-neck flask with a stirrer, introducing nitrogen, starting a stirring device, heating to 105-155 ℃, after the two are uniformly mixed, dripping 0.1-0.9 wt.% of tetraisopropyl titanate (TPT), wherein the use amount of the TPT is 0.1-0.9% of the weight of the organosilicon intermediate, controlling the rotating speed at 400-1000 r/min, stopping stirring after reacting for 5-12 hours, and taking out a reaction Product (PES) for later use. And adding 10-40 parts of PES prepolymer into 100 parts of liquid silicone rubber matrix, uniformly mixing at 100 ℃, and cooling to obtain the silicone rubber.
In table 1, the curing agent is a silane coupling agent; the catalyst is an organic tin compound.
2. Preparation method
Weighing the raw materials according to the weight ratio, gradually adding a small amount of white carbon black (gradually adding a small amount of white carbon black in batches) into the silicon rubber, and mechanically stirring until the mixture is substantially uniform; then, mixing for a certain time by using a three-roller grinding machine to uniformly disperse the white carbon black in the silicon rubber; sequentially and gradually adding the PBO fiber, the ammonium sulfate, the ammonium borate, the pentaerythritol and the curing agent in corresponding proportions (adding the other component after adding the same component and uniformly mixing) into the silicon rubber and white carbon black mixture, uniformly mixing the mixture by using a laboratory miniature kneader for a certain time, finally adding the catalyst with corresponding content, mixing for 1-5 minutes, putting the mixture into a mold, vulcanizing the mixture in a flat vulcanizing machine for 8-36 hours (room temperature, 5-15 MPa), demolding and sampling, and standing the mixture at room temperature for one week to completely cure the mixture to obtain the composite material.
3. Examples 1-5 preparation of Flexible ablation-resistant composites
According to the raw material ratios shown in table 1 and the preparation method described in the example "2", the flexible ablation-resistant composite materials of the examples 1 to 5 were prepared, and the flexible ablation-resistant composite materials prepared in the examples 1 to 5 were named N1, N2, N3, N4 and N5, respectively.
Comparative example 1 preparation of composite Material
1. Raw material ratio
100 parts of silicon rubber, 3 parts of curing agent and 0.2 part of catalyst. The types of silicone rubber, curing agent and catalyst were the same as in the examples.
2. Preparation method
Weighing the raw materials according to the proportion, adding a curing agent into silicon rubber, uniformly stirring, adding a catalyst with corresponding content, mixing for 1-5 minutes, placing the mixture into a vacuum oven, vacuumizing to remove bubbles, placing the mixture into a mold, vulcanizing in a flat vulcanizing machine for 8-36 hours (the vulcanization temperature is room temperature, and the pressure is 5-15 MPa), demolding, sampling, and standing at room temperature for one week to completely cure the mixture. The resulting flexible ablation-resistant composite was designated Pure.
Comparative example 2 preparation of composite Material
1. Raw material ratio
100 parts of silicon rubber, 15 parts of white carbon black, 12 parts of PBO fiber, 3 parts of curing agent and 0.2 part of catalyst. Wherein, the types of the silicon rubber, the white carbon black, the PBO fiber, the curing agent and the catalyst are the same as the examples.
2. Preparation method
Weighing the raw materials according to the proportion, gradually adding a small amount of white carbon black (gradually adding a small amount of white carbon black in batches) into the silicon rubber, and mechanically stirring until the mixture is substantially uniform; then, mixing for a certain time by using a three-roller grinding machine to uniformly disperse the white carbon black in the silicon rubber; sequentially and gradually adding the PBO fiber and the curing agent in corresponding proportion (adding another component after adding the same component and uniformly mixing) into the silicon rubber and white carbon black mixture, uniformly mixing the mixture by using a laboratory miniature kneader for a certain time, finally adding the catalyst with corresponding content, mixing the mixture for 1 to 5 minutes, putting the mixture into a mold, vulcanizing the mixture in a flat vulcanizing machine for 8 to 36 hours (room temperature, 5 to 15MPa), demolding and sampling, and standing the mixture at room temperature for one week to completely cure the mixture to obtain the PBO fiber and the curing agent. The resulting flexible ablation-resistant composite was designated S0.
The advantageous effects of the present invention are described below by way of test examples.
Test example 1 examination of ablation resistance of Flexible ablation-resistant composite Material according to the present invention
1. Test method
The composite materials prepared in examples 1-5 and comparative examples 1-2 were tested for their ablation resistance. The ablation resistance is tested by adopting an oxyacetylene ablation testing device, the surface of the sample is vertically blasted by adopting oxyacetylene flame, the ablation time is 30s, the ablation temperature is more than 2700 ℃, the sample is naturally cooled to the normal temperature after ablation is finished, and a surface carbon layer is stripped. The thickness change of the sample before and after the experiment was measured, and the line ablation rate of the sample was calculated. The calculation formula is as follows:
LAR＝Δd/t＝(d1-d2)/t
LAR-ablation rate of sample wire, mm/s;
d 1-original thickness of specimen, mm;
d 2-thickness of sample after ablation, mm;
t-ablation time, s.
The surface and cross-sectional morphology of the composites of examples 1-5 after ablation were observed using an optical microscope and a Scanning Electron Microscope (SEM).
The carbon layer peeled off from the composite material of examples 1 to 5 after ablation was pulverized in a mortar and subjected to X-ray diffraction (XRD) (DY1291, Philips, Netherlands) analysis in such a manner that 2 θ was in the range of 5 to 85 °.
2. Test results
The line ablation rate results for the different composites are shown in fig. 1 and table 2; the optical appearance of the surface of the composite material after ablation is shown in FIG. 2; SEM pictures of the surface and cross-section of the composite after ablation are shown in fig. 3 and 4. The XRD results of the composite material after ablation are shown in fig. 5.
TABLE 2 line ablation Rate of different flexible ablation-resistant composites of the invention
As can be seen from fig. 1 and table 2, the flexible ablation-resistant composite material prepared according to the present invention has a low ablation rate, and the ablation rate of the flexible ablation-resistant composite material prepared according to the present invention is significantly reduced compared to comparative examples 1 and 2. As shown by the dashed lines in fig. 1, for the optimal combination N5 (line ablation rate minimum), the line ablation rate was reduced by 79.84% and 36.82% compared to Pure and S0, respectively. The smaller the line ablation rate means the better ablation performance, and for the ablation-resistant material, after the high-temperature-resistant fiber is added, the further obvious reduction of the line ablation rate is difficult, and the obvious reduction shows that the ablation resistance of the composite material is obviously improved when the composite material is optimally combined. The test result shows that the flexible ablation-resistant composite material prepared by the invention has good ablation resistance, and compared with the composite material prepared by the comparative example, the ablation resistance is obviously improved.
FIG. 2 is a graph of optical topography of various groups of flexible ablation-resistant composites of the present invention after ablation, wherein the layers (a-e) (a 'to e') (a '-e') of FIG. 2 correspond to the profile of the side, surface and carbon layers after ablation of the various groups of composites, respectively, a 'and a' represent N1, b 'and b' represent N2, c 'and c' represent N3, d 'and d' represent N4, and e, e 'and e' represent N5. From fig. 2 (a-e), it can be seen that after the flexible ablation-resistant composite material prepared by the invention is ablated for 30 seconds, only a thin layer on the surface is damaged, and a carbon layer with good strength is formed; it can be seen from fig. 2(a 'b') (a ". b") that the central region of the carbon layer exhibits a denser structure than the edges 30 seconds after composite ablation. As can be seen from fig. 5, after the flexible ablation-resistant composite material prepared by the present invention is ablated, the carbon layer is mainly composed of SiC ceramic material and graphite. As can be seen from the SEM images of fig. 3 and 4, the carbon layer has a microporous structure, and the microporous structure is favorable for reducing the thermal conductivity of the carbon layer, so as to reduce the line ablation rate of the composite material, i.e., improve the ablation performance of the composite material.
The above results show that the flexible ablation-resistant composite material of the invention has good ablation resistance, and the composite material with the optimal ablation resistance comprises 100 parts of silicone rubber, 15 parts of white carbon black, 12 parts of PBO fiber, 40 parts of ammonium sulfate, 40 parts of ammonium borate, 10 parts of pentaerythritol, 3 parts of curing agent and 0.2 part of catalyst.
Test example 2 research on thermal conductivity of flexible ablation-resistant composite material
1. Test method
The flexible ablation-resistant composite material prepared in examples 1-5 was tested for thermal conductivity. The thermal conductivity of the flexible ablation-resistant composite material is measured by a thermal conductivity tester (Hot Disk TPS 2500, Sweden), and a thermocouple probe is used as a heat source and a temperature sensor at the same time.
2. Test results
The thermal conductivity of the flexible ablation-resistant composite of the present invention is shown in fig. 6 and table 3, and the results for the maximum back-plate temperature are shown in fig. 7 and table 4.
TABLE 3 thermal conductivity results for flexible ablation-resistant composites of the invention
Table 4 maximum backplane temperature results for flexible ablation-resistant composites of the invention
The result of the heat conductivity of the flexible ablation-resistant composite material of the invention shows that: the composite material system has lower heat conductivity and backboard temperature, the low heat conductivity can effectively delay or inhibit the invasion of external heat, can play a good role in protecting internal materials, reduces the linear ablation rate of the composite material, and improves the ablation resistance of the composite material; meanwhile, the low thermal conductivity can reduce the temperature of the back plate of the composite material, and the thermal damage of the target protective material is avoided. Therefore, the flexible ablation-resistant composite material has good ablation resistance.
In conclusion, the flexible ablation-resistant composite material prepared by the invention has excellent heat resistance and ablation resistance and good heat insulation performance, can be used for preparing ablation heat-resistant materials and parts with the requirements on heat resistance and ablation resistance, and is applied to the protection and sealing of structures and parts which need to withstand high-temperature gas, pneumatic heat flow scouring and other severe environments in aerospace aircrafts and related equipment.
Claims (8)
1. A preparation method of a flexible ablation-resistant composite material of a three-source expansion micro-foaming flame-retardant system is characterized by comprising the following steps: the flexible ablation-resistant composite material is prepared from the following raw materials in parts by weight:
100 parts of silicon rubber, 15 parts of white carbon black, 12 parts of fiber, 40 parts of acid source substance, 40 parts of gas source substance, 10 parts of carbon source substance, 3 parts of curing agent and 0.2 part of catalyst;
the acid source substance is ammonium sulfate; the gas source substance is ammonium borate; the carbon source substance is pentaerythritol.
2. The method of claim 1, wherein: the silicon rubber is room temperature vulcanized liquid silicon rubber modified by epoxy resin.
3. The method of claim 2, wherein: the preparation method of the epoxy resin modified room temperature vulcanized liquid silicone rubber comprises the following steps:
(1) heating epoxy resin and an organic silicon intermediate in an equimolar ratio to 105-155 ℃ under the condition of nitrogen, stirring, dripping 0.1-0.9 wt.% tetraisopropyl titanate after uniformly stirring, and stirring for 5-12 hours to obtain a reaction product;
(2) and adding 10-40 parts of the reaction product into 100 parts of a liquid silicone rubber matrix, uniformly mixing at 100 ℃, and cooling to obtain the silicone rubber.
4. The production method according to claim 3, characterized in that: in the step (1), the epoxy resin is bisphenol A type epoxy resin; the organosilicon intermediate is polymethylphenylsiloxane; and/or in the step (1), the amount of the tetraisopropyl titanate is 0.1-0.9% of the weight of the organosilicon intermediate; and/or in the step (1), the rotating speed of stirring is 400-1000 r/min.
5. The method of claim 1, wherein: the fiber is aramid fiber, PBO fiber, quartz fiber or carbon fiber; the curing agent is a silane coupling agent; the catalyst is an organic tin compound.
6. The method of claim 5, wherein: the fibers are PBO fibers.
7. The production method according to any one of claims 1 to 6, characterized in that: the preparation method comprises the following steps:
(a) weighing the raw materials according to the weight ratio of claim 1;
(b) gradually adding a small amount of white carbon black into the silicone rubber, and uniformly mixing to obtain a silicone rubber white carbon black mixture; then sequentially and gradually adding the fiber, the acid source substance, the gas source substance, the carbon source substance and the curing agent into the silicon rubber and white carbon black mixture, and uniformly mixing; finally, adding a catalyst, mixing for 1-5 min, and uniformly mixing to obtain uniformly mixed raw materials;
(c) and putting the uniformly mixed raw materials into a mold, vulcanizing, demolding, sampling, and standing at room temperature for a week to completely cure the raw materials to obtain the product.
8. The method of claim 7, wherein: in the step (b), the stepwise small-amount addition is a stepwise small-amount addition in small portions; and/or, in the step (b), the step-by-step adding in sequence means that after each same component is added, the other component is added after the same components are uniformly mixed; and/or in the step (c), vulcanizing in a vulcanizing press for 8-36 hours at room temperature and under the vulcanizing pressure of 5-15 MPa.
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| CN104629374A (en) * | 2015-01-22 | 2015-05-20 | 东北大学 | Silicone rubber based ablation-resisting heat insulation composite material and preparation method thereof |
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| CN106046386A (en) * | 2016-08-08 | 2016-10-26 | 四川大学 | Epoxy resin-organosilicon polymer and preparation method and application thereof |
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| CN104629374A (en) * | 2015-01-22 | 2015-05-20 | 东北大学 | Silicone rubber based ablation-resisting heat insulation composite material and preparation method thereof |
| CN105111748A (en) * | 2015-07-31 | 2015-12-02 | 沈阳理工大学 | Hot vulcanized silicone rubber/boron phenol-formaldehyde resin based erosion-resisting material and preparation method therefor |
| CN106046386A (en) * | 2016-08-08 | 2016-10-26 | 四川大学 | Epoxy resin-organosilicon polymer and preparation method and application thereof |
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